4-Fluoro-3-nitrobenzotrifluoride → 1-(Tetrahydropyran-4-yl)amino-2-nitro-4-trifluoromethylbenzene

HRID 74150

반응식

HRID 74150 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[NH2:15][CH:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1>N1C=CC=CC=1>[O:19]1[CH2:20][CH2:21][CH:16]([NH:15][C:2]2[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][C:3]=2[N+:12]([O-:14])=[O:13])[CH2:17][CH2:18]1

참가 물질

4

반응물 2

HCID 677784-Fluoro-3-nitrobenzotrifluorideHCID 4192234-Aminotetrahydropyran

생성물 1

HCID 185098281-(Tetrahydropyran-4-yl)amino-2-nitro-4-trifluoromethylbenzene수율 90.6%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
98 °C

실험 절차

A 3-neck flask (200 mL) was charged with 1-fluoro-2-nitro-4-trifluoromethylbenzene (1.59 g, 7.61 mmol), 4-aminotetrahydropyran (1.00 g, 9.89 mmol), and pyridine (16 mL), and this was stirred at 98° C. for 23 hours. The yellow oil produced was allowed to cool, distilled water (approx. 20 mL) was added with stirring, and the precipitated crystals were filtered off. These were washed with distilled water and dried with heating at reduced pressure to yield the title compound (2.00 g, 90.5% yield) as yellow crystals.

후처리

  1. customThe yellow oil produced
  2. temperatureto cool
  3. distillationdistilled water (approx. 20 mL)
  4. additionwas added
  5. stirringwith stirring
  6. filtrationthe precipitated crystals were filtered off
  7. washThese were washed with distilled water
  8. customdried
  9. temperaturewith heating at reduced pressure

출처 및 근거

ORD 기록
ord-359360c049ef4f41afd2e711efcfdd3b
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829035B2

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